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An Unexplored Realm in the Heartland of the Southern Gulf ... - Famsi

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Laboratory Procedures<br />

A total <strong>of</strong> 177 specimens were used <strong>in</strong> <strong>the</strong> weak acid-extraction ICP–OES<br />

analysis, 87 from Plaza I (Figure 4.26) and 90 from Plaza II (Figure 4.27). The location<br />

<strong>of</strong> <strong>the</strong>se specimens is identified by a red diamond on <strong>the</strong> grid maps. Each sample was<br />

prepared for analysis by James Hawk<strong>in</strong> and Claire Novotny <strong>of</strong> <strong>the</strong> University <strong>of</strong> South<br />

Florida, Department <strong>of</strong> <strong>An</strong>thropology, under <strong>the</strong> direction <strong>of</strong> Dr. E. Christian Wells. Each<br />

sample was homogenized through thorough mix<strong>in</strong>g, and a 2.0 g sample was weighed out.<br />

The f<strong>in</strong>e consistency <strong>of</strong> <strong>the</strong> soil precluded <strong>the</strong> need for siev<strong>in</strong>g or pulveriz<strong>in</strong>g. The sample<br />

was mixed <strong>in</strong> a polyethylene vial with 20 mL <strong>of</strong> extract composed <strong>of</strong> 50 mL HC1, 10 mL<br />

HNO3, and diluted with 1000 mL <strong>of</strong> Type II deionized H2O (0.60 M HC1 + 0.16 M<br />

HNO3). Sample mixtures were highly agitated for 30 m<strong>in</strong>utes on an electric platform<br />

shaker at 200 rpm. The solution was <strong>the</strong>n filtered through ashless filter paper and<br />

decanted <strong>in</strong>to a clean polyethylene vial. The mild acid extraction method was used<br />

because recent studies have demonstrated this procedure illustrates <strong>the</strong> anthropogenic<br />

components <strong>in</strong> <strong>the</strong> soils (Burton and Simpson 1993; Middleton and Price 1996).<br />

The prepared samples were sent to <strong>the</strong> Paleoclimatology, Paleoceanography and<br />

Biogeochemistry Laboratory at <strong>the</strong> University <strong>of</strong> South Florida’s College <strong>of</strong> Mar<strong>in</strong>e<br />

Science on <strong>the</strong> St. Petersburg Campus. There <strong>the</strong> samples were analyzed us<strong>in</strong>g a Perk<strong>in</strong>-<br />

Elmer 4300-DV ICP-OES (Dual View Inductively Coupled Plasma-Optical Emission<br />

Spectrometer) equipped with a cyclonic spray chamber and Me<strong>in</strong>hard C3 High-Solids<br />

nebulizer. The equipment was calibrated us<strong>in</strong>g known solution standards for elements <strong>of</strong><br />

<strong>in</strong>terest.<br />

162

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